CN103880792A - Method for producing furfural through hydrolysis by using high-pressure two-kettle-cascade acid process - Google Patents
Method for producing furfural through hydrolysis by using high-pressure two-kettle-cascade acid process Download PDFInfo
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- CN103880792A CN103880792A CN201410059176.4A CN201410059176A CN103880792A CN 103880792 A CN103880792 A CN 103880792A CN 201410059176 A CN201410059176 A CN 201410059176A CN 103880792 A CN103880792 A CN 103880792A
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- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 98
- 230000007062 hydrolysis Effects 0.000 title claims abstract description 97
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000002253 acid Substances 0.000 title claims abstract description 13
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 7
- 150000001299 aldehydes Chemical class 0.000 claims description 21
- 241000196324 Embryophyta Species 0.000 claims description 11
- 239000002657 fibrous material Substances 0.000 claims description 9
- 240000008042 Zea mays Species 0.000 claims description 8
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims description 8
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 8
- 235000005822 corn Nutrition 0.000 claims description 8
- 239000012530 fluid Substances 0.000 claims description 6
- 235000011149 sulphuric acid Nutrition 0.000 claims description 5
- 239000001117 sulphuric acid Substances 0.000 claims description 5
- 230000003301 hydrolyzing effect Effects 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000010924 continuous production Methods 0.000 abstract description 2
- 239000000835 fiber Substances 0.000 abstract 3
- 238000000605 extraction Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 4
- 239000007858 starting material Substances 0.000 description 4
- 238000007670 refining Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 240000006677 Vicia faba Species 0.000 description 1
- 235000010749 Vicia faba Nutrition 0.000 description 1
- 235000002098 Vicia faba var. major Nutrition 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 235000019628 coolness Nutrition 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- -1 heterocyclic organic compound Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/38—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with substituted hydrocarbon radicals attached to ring carbon atoms
- C07D307/40—Radicals substituted by oxygen atoms
- C07D307/46—Doubly bound oxygen atoms, or two oxygen atoms singly bound to the same carbon atom
- C07D307/48—Furfural
- C07D307/50—Preparation from natural products
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a method for producing furfural through hydrolysis by using a high-pressure two-kettle-cascade acid process. The method comprises the steps of feeding a plant fiber raw material and 5-8% dilute sulfuric acid into hydrolysis kettles after uniformly mixing, introducing 1.3Mpa saturated steam to perform hydrolysis, and extracting furfural produced in the process of hydrolysis with the 1.3Mpa saturated steam, wherein the two-kettle-cascade acid process is adopted in the process, namely, three hydrolysis kettles form a group, two of the hydrolysis kettles are connected in series along the flow direction of the saturated steam, and the other hydrolysis kettle is kept in a removed state and is filled with the plant fiber raw material; after the hydrolysis of the two hydrolysis kettles is completed, the hydrolysis kettle subjected to twice hydrolysis is removed and is filled with the plant fiber raw material, and the other two hydrolysis kettles are connected in series and are communicated with the saturated steam to perform hydrolysis and extraction so as to realize the stable and continuous production of crude furfural. The method disclosed by the invention has the beneficial effects that (1) the utilization rate of equipment is increased by 30%; (2) the furfural yield is improved by about 5%; and (3) the steam cascade process is simplified and the labor cost is reduced.
Description
Technical field
The invention belongs to chemical industry furfural production field, the technique that particularly furfural is produced in a kind of high pressure two still string acid system hydrolysis.
Background technology
Furfural has another name called furtural, is a kind of important heterocyclic organic compound, and the Chemicals that directly or indirectly derive taking furfural as raw material reach kind more than 1600, are widely used in the industry such as medicine, agricultural chemicals, resin, daily use chemicals, casting, weaving and oil.
First furfural production is the preparation of chaff aldehyde, is then the purification of chaff aldehyde.China is mainly that chaff aldehyde is produced in acid system hydrolysis.Use certain density dilute sulphuric acid as catalyzer, the saturation steam of specified pressure is added in hydrolysis kettle, complete hydrolysis and the dehydration of the pentosan in plant fiber material, thereby generate furfural.Meanwhile, utilize mobile saturation steam to complete the proposition of furfural.
At present, in China's production process, great majority are pressed (0.5-0.8Mpa saturation steam) 3 hydrolysis kettle series connection hydrolysis production technology in adopting, most of production line uses 12 hydrolysis kettles in the hydrolysis cycle of preparing chaff aldehyde, be divided into 3 groups, in every group, extract 1 hydrolysis kettle charging feedstock, other 3 hydrolysis kettle series connection are used, and then 12 3 groups of in parallel uses that hydrolysis kettle is divided into, to realize the continuous production of thick aldehyde.
This technique it seems now and exists many shortcomings, and production efficiency is low, and plant factor is not high, and furfural yield is lower; And operating procedure complexity, cost of labor is higher.
Summary of the invention
The object of the invention is to, overcome the deficiencies in the prior art, a kind of two still string acid systems hydrolysis furfural production technologies taking high-pressure saturated steam as basis are provided, conventional at present for substituting, but three a lot of still string acid systems hydrolysis furfural production technologies of drawback.
Technical scheme of the present invention is such:
A kind of high pressure two still string acid system hydrolysis furfural production methods, comprise that step is as follows: be to send into hydrolysis kettle after 5%-8% dilute sulphuric acid evenly mixes by plant fiber material and mass percent, pass into 1.3Mpa saturation steam and be hydrolyzed, the furfural producing in hydrolytic process proposes with 1.3Mpa saturation steam; Wherein, in this process, adopt two still string acid systems, i.e. one group of 3 hydrolysis kettle, wherein 2 flow to series connection according to saturation steam and enter, and another 1 keeps excision state, pack plant fiber material into, after 2 hydrolysis kettle hydrolysis, the hydrolysis kettle that is hydrolyzed twice is extractd, pack plant fiber material into, other two saturation steams of connecting and be communicated with are hydrolyzed and propose, and produce with the steady and continuous that realizes chaff aldehyde.
Preferably, the reaction conditions of described hydrolysis is temperature 180-200 DEG C.
Preferably, described hydrolysis kettle is of a size of height 9m, diameter 2.0m.
Preferably, described saturation steam is provided by steam boiler.
Preferably, the pressure of described saturation steam is stable.This is hydrolysis and dehydration stable process conditions in order to ensure pentosan in hydrolysis kettle, and speed of reaction is stable, keeps furfural gas concentration in hydrolysis kettle to stablize.
Preferably, in the hydrolysis kettle of described 2 series connection, saturation steam is entered by the bottom of First hydrolysis kettle, draw from top and (now steam, contain furfural gas with pipeline, be called aldehyde vapour) after enter the bottom of second hydrolysis kettle, then enter original fluid container through pipeline through condensation by the top of second hydrolysis kettle.
Preferably, described plant fiber material is corn cob.
The invention has the beneficial effects as follows:
(1) plant factor of raising 30%.The three still series connection modes of production need 12 hydrolysis kettles could form a stable furfural production line, and 2 still series connection only need 9 hydrolysis kettles to complete;
(2) improve approximately 15% furfural yield.2 stills series connection effectively reduce the working time of furfural steam in pipeline, thereby have shortened the time of furfuryl resin, have improved furfural yield;
(3) simplify string vapour program and reduced cost of labor.
Additional aspect of the present invention and advantage in the following description part provide, and part will become obviously from the following description, or recognize by practice of the present invention.
Brief description of the drawings
Above-mentioned and/or additional aspect of the present invention and advantage accompanying drawing below combination is understood becoming the description of embodiment obviously and easily, wherein:
Fig. 1 is process flow sheet of the present invention.
In figure: 1-starting material, 2-rotary strainer, 3-pulverizer, 4-lift, 5-string vapour platform, 6-hydrolysis kettle, 7-original fluid container, 8-condenser, 9-primary tower, 10-condenser, 11-phase splitter, 12-refines workshop, 13-essence aldehyde storage tank.
Embodiment
Be exemplary below by the embodiment being described with reference to the drawings, only for explaining the present invention, and can not be interpreted as limitation of the present invention.
Below with reference to Fig. 1, the high pressure two still string acid system hydrolysis furfural production methods according to the embodiment of the present invention are described.
The inventive method equipment therefor comprises rotary strainer 2, pulverizer 3, lift 4, string vapour platform 5, hydrolysis kettle 6, original fluid container 7, condenser 8, primary tower 9, condenser 10, phase splitter 11, refining workshop 12 and smart aldehyde storage tank 13.Wherein, starting material 1 are connected with rotary strainer 2, rotary strainer 2 is connected with pulverizer 3, pulverizer 3 is connected with lift 4, lift 4 is connected with top feed bin, and top feed bin is connected with 3 hydrolysis kettles by travelling belt, and 3 hydrolysis kettles are respectively hydrolysis kettle 61,2, No. 3, each hydrolysis kettle 6 is of a size of height 9m, diameter 2.0m.No. 2 hydrolysis kettles of No. 1 hydrolysis kettle series connection between 3 hydrolysis kettles 6, No. 3 hydrolysis kettles of No. 2 hydrolysis kettle series connection, No. 1 hydrolysis kettle of No. 3 hydrolysis kettle series connection.Wherein, series connection refers to enter the bottom of second hydrolysis kettle after saturation steam is drawn by the top of first hydrolysis kettle, then is drawn by the top of second hydrolysis kettle.The bottom of 3 hydrolysis kettles 6 connects respectively string vapour platform 5, and string vapour platform 5(string vapour platform 5 also can be called valving), string vapour platform 5 connects saturation steam.The top of 3 hydrolysis kettles 6 all connects condenser 8, and condenser 8 is connected with smart aldehyde storage tank 13 with original fluid container 7, primary tower 9, condenser 10, phase splitter 11, refining workshop 12 successively.
Starting material 1 corn cob is removed dust through rotary strainer 2, then enter the particle (particle size range is 0.5-1.2cm) that pulverizer 3 is pulverized as broad bean size, be promoted to device top feed bin through lift 4, with mass percent be that 6% dilute sulphuric acid is mixed thoroughly and sent in No. 3 hydrolysis kettles of having extractd from steam flow stand-by through conveying belt.
Now No. 1 hydrolysis kettle of this group is just connected with No. 2 hydrolysis kettles, and No. 2 conducts go out the state of aldehyde still as steam still to present No. 1.The mixture of corn cob and 6% dilute sulphuric acid has now been housed in No. 1 hydrolysis kettle in advance, pass into 1.3Mpa saturation steam and be hydrolyzed, saturation steam is provided by steam boiler, and it is stable that pressure keeps, hydrolysising reacting temperature is 180 DEG C, and the furfural producing in hydrolytic process proposes with 1.3Mpa saturation steam.When after the pentosan hydrolysis complete (after 2 hours) in starting material in No. 1 hydrolysis kettle, in still, aldehyde gas concentration enters the dense stage of tail (the dense stage of tail is the more and more lower stage of last aldehyde vapour concentration), extracts (closing) No. 1 hydrolysis kettle and drops into No. 3 hydrolysis kettles.Present the working order of No. 3 stills of No. 2 still strings, the high-pressure saturated steam coming from combustion slag boiler enters from No. 2 hydrolysis kettle bottom steam pipelines, draw from overhead vapor pipeline, enter hydrolysis kettle No. 3 from bottom through No. 3 hydrolysis kettle steam-pipes, then introduce condenser from overhead vapor pipeline.
No. 1 hydrolysis kettle of extracing is filled after raw material, waits for that No. 2 hydrolysis kettles put into operation while excision, present the working order of No. 1 still of No. 3 still strings.Like this, 3 hydrolysis kettles in this group, through the valve regulated (reasonably opening corresponding valve) of string vapour platform 5, total energy keeps 1 in extracing the state of charging feedstock, and other 2 are in the state moving in system.Through No. 2, No. 1 string, No. 3, No. 2 strings, No. 3 strings are realized the circulation of the interior hydrolysis kettle of this group for No. 1.
Enter condenser 8 coolings containing aldehyde steam and transfer the liquid chaff aldehyde stoste that forms to and enter original fluid container 7 from what draw in hydrolysis kettle, after buffering, enter primary tower 9 and promote concentration, form the more than 90% chaff aldehyde of concentration by condenser 10, then enter refining link and purify, produce qualified smart furfural.
Contrast experiment: taking every 11 tons of corn cob gained furfurals as example, keep other condition constant, use respectively 0.8,1.0,1.2,1.3,1.4 vapor pressure, and 3 still strings and 2 still strings, the method for contrast the present embodiment is tested, and furfural yield is as following table.
The concrete data of 3 still 2 still strings and the furfural yields such as 0.8,1.0
| Vapor pressure (Mpa) | 3 still string furfurals must be measured (T) | Common 2 still strings must be measured (T) | Our factory 2 still string furfurals must be measured (T) |
| 0.8 | 1.0 | 0.9 | 0.9 |
| 1.0 | 0.98 | 0.95 | 1.0 |
| 1.2 | 0.95 | 0.90 | 1.0 |
| 1.3 | 0.94 | 0.85 | 1.15 |
| 1.4 | 0.8 | 0.84 | 1.0 |
Conclusion: originally 0.8Mpa pressure 3 still series connection, 1 ton of furfural of 11 tons of corn cobs, with the series connection of the present embodiment 1.3Mpa2 still, 11 tons of corn cobs can obtain 1.15 tons of furfurals, improve 15% furfural yield.
The present invention utilizes the cooperation of 1.3 MPa vapor pressures and the series connection of 2 stills, and can be combined with the size of specific hydrolysis kettle, conventional production adopts the reason of 3 still strings to be: the concentration of corn cob furfural steam in hydrolytic process is also unstable, concentration is that first low rear height is low again, if aldehyde vapour concentration is unstable, affect the separating effect of primary tower.If be hydrolyzed in employing high pressure steam, hydrolysis rate is accelerated, and 3 still strings make furfural loss strengthen (resinifying) and simply use standardized hydrolysis kettle+2 still string, can cause: 1, steam consumption quantity is large 2, aldehyde vapour concentration is unstable.The hydrolysis kettle size that our factory adopts is the best fit that uses highly pressured hydrolysis+2 still series connection, and advantage has: 1, aldehyde vapour concentration stabilize; 2, aldehyde vapour stroke is short, and resinifying loss is little; 3, hydrolysis time is short, with short production cycle, and same equipment yield is large; 4, energy consumption of unit product is low.
Although illustrated and described embodiments of the invention, those having ordinary skill in the art will appreciate that: in the situation that not departing from principle of the present invention and aim, can carry out multiple variation, amendment, replacement and modification to these embodiment, scope of the present invention is limited by claim and equivalent thereof.
Claims (7)
1. high pressure two still string acid system hydrolysis furfural production methods, it is characterized in that, comprise that step is as follows: after plant fiber material is evenly mixed with 5%-8% dilute sulphuric acid, send into hydrolysis kettle, pass into 1.3Mpa saturation steam and be hydrolyzed, the furfural producing in hydrolytic process proposes with 1.3Mpa saturation steam; Wherein, in this process, adopt two still string acid systems, i.e. one group of 3 hydrolysis kettle, wherein 2 flow to series connection according to saturation steam and enter, and another 1 keeps excision state, pack plant fiber material into, after 2 hydrolysis kettle hydrolysis, the hydrolysis kettle that is hydrolyzed twice is extractd, pack plant fiber material into, other two saturation steams of connecting and be communicated with are hydrolyzed and propose, and produce with the steady and continuous that realizes chaff aldehyde.
2. production method according to claim 1, is characterized in that, the reaction conditions of described hydrolysis is temperature 180-200 DEG C.
3. production method according to claim 1, is characterized in that, described hydrolysis kettle is of a size of height 9m, diameter 2.0m.
4. production method according to claim 1, is characterized in that, described saturation steam is provided by steam boiler.
5. production method according to claim 1, is characterized in that, the pressure of described saturation steam is stable.
6. production method according to claim 1, it is characterized in that, in the hydrolysis kettle of described 2 series connection, saturation steam is entered by the bottom of First hydrolysis kettle, from draw on top, enter the bottom of second hydrolysis kettle with pipeline, then enter original fluid container through pipeline through condensation by the top of second hydrolysis kettle.
7. production method according to claim 1, is characterized in that, described plant fiber material is corn cob.
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| CN201410059176.4A CN103880792A (en) | 2014-02-21 | 2014-02-21 | Method for producing furfural through hydrolysis by using high-pressure two-kettle-cascade acid process |
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| CN201410059176.4A CN103880792A (en) | 2014-02-21 | 2014-02-21 | Method for producing furfural through hydrolysis by using high-pressure two-kettle-cascade acid process |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106432146A (en) * | 2016-09-07 | 2017-02-22 | 河北科技大学 | Equipment for manufacturing furfural from corncobs |
| CN110247064A (en) * | 2019-06-26 | 2019-09-17 | 中国林业科学研究院林产化学工业研究所 | A kind of fast-growing paper mulberry prepares the new method of catalytic oxidation-reduction reaction (ORR) active carbon |
| CN115536620A (en) * | 2022-10-11 | 2022-12-30 | 河南省生物基材料产业研究院有限公司 | System and method for continuously producing furfural and 5-hydroxymethyl furfural by cellulose biomass |
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| CN1803785A (en) * | 2006-01-23 | 2006-07-19 | 济南圣泉集团股份有限公司 | Method for preparing furfural by utilizing cotton stalk |
| CN1858044A (en) * | 2006-06-07 | 2006-11-08 | 济南圣泉集团股份有限公司 | Method for producing furol by plant stalk pelletizing |
| CN102766120A (en) * | 2012-08-14 | 2012-11-07 | 河南省科学院高新技术研究中心 | Gas phase acid catalytic biomass hydrolysis continuous production method of furfural |
| WO2013025564A2 (en) * | 2011-08-12 | 2013-02-21 | E. I. Du Pont De Nemours And Company | Furfural production from biomass |
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2014
- 2014-02-21 CN CN201410059176.4A patent/CN103880792A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1803785A (en) * | 2006-01-23 | 2006-07-19 | 济南圣泉集团股份有限公司 | Method for preparing furfural by utilizing cotton stalk |
| CN1858044A (en) * | 2006-06-07 | 2006-11-08 | 济南圣泉集团股份有限公司 | Method for producing furol by plant stalk pelletizing |
| WO2013025564A2 (en) * | 2011-08-12 | 2013-02-21 | E. I. Du Pont De Nemours And Company | Furfural production from biomass |
| CN102766120A (en) * | 2012-08-14 | 2012-11-07 | 河南省科学院高新技术研究中心 | Gas phase acid catalytic biomass hydrolysis continuous production method of furfural |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106432146A (en) * | 2016-09-07 | 2017-02-22 | 河北科技大学 | Equipment for manufacturing furfural from corncobs |
| CN110247064A (en) * | 2019-06-26 | 2019-09-17 | 中国林业科学研究院林产化学工业研究所 | A kind of fast-growing paper mulberry prepares the new method of catalytic oxidation-reduction reaction (ORR) active carbon |
| CN110247064B (en) * | 2019-06-26 | 2023-01-20 | 中国林业科学研究院林产化学工业研究所 | Novel method for preparing catalytic Oxygen Reduction Reaction (ORR) activated carbon by fast-growing broussonetia papyrifera |
| CN115536620A (en) * | 2022-10-11 | 2022-12-30 | 河南省生物基材料产业研究院有限公司 | System and method for continuously producing furfural and 5-hydroxymethyl furfural by cellulose biomass |
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